空心Fe3O4纳米微球的制备及超顺磁性

李文宇; 霍格; 黄岩; 董丽娟; 卢学刚

doi:10.7498/aps.67.20180579

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摘要

采用水热控制合成法，以六水三氯化铁、柠檬酸三钠和尿素为原料，聚丙烯酰胺为稳定剂，200 ℃下反应12 h制备得到了超顺磁性空心Fe3O4纳米微球.通过X射线衍射仪、扫描电子显微镜、透射电子显微镜对样品的结构和形貌进行表征，并采用振动样品磁强计测试了样品的磁性能.结果表明：所得样品为具有尖晶石结构的Fe3O4纳米微球，尺寸为160 nm 左右，呈分等级结构，即整个微球由粒径约18 nm 的初级晶粒自组装堆叠而成；室温下表现为典型的超顺磁性，且饱和磁化强度为73.3 emu/g （1 emu/g=1 A m2/kg），这种高饱和磁化强度可以由其初级晶粒晶化程度高且粒径较大以及这种特殊的二次自组装结构进行解释.这种Fe3O4纳米微球为疏松多孔的空心球状结构，具有粒径分布均匀、分散性良好和超顺磁性的特点，在药物靶向输运和肿瘤热疗中有潜在的应用.

关键词:

作者及机构信息

1.
山西大同大学固体物理研究所, 大同 037009;

2.
西安交通大学理学院, 物质非平衡合成与调控教育部重点实验室, 西安 710049;

3.
深圳大学材料学院, 深圳 518061

通信作者: 卢学刚, xglu@xjtu.edu.cn

基金项目: 国家自然科学基金（批准号：51172178）资助的课题.

参考文献

[1]	Zhu M Y, Liu C, Bo W Q, Hu J W, Hu Y H, Jin H M, Wang S W, Li Y 2012 Acta Phys. Sin. 61 078106 (in Chinese)[朱明原, 刘聪, 薄伟强, 舒佳武, 胡业昊, 金红明, 王世伟, 李瑛 2012 物理学报 61 078106]
[2]	Zheng X C, Li X Y, He L H, et al. 2017 Chin. Phys. B 26 037502
[3]	Gholizadeh A, Jafari E 2017 J. Magn. Magn. Mater. 422 328
[4]	Liu R, Yang S C, Wang F, et al. 2012 ACS Appl. Mater. Inter. 4 1537
[5]	Lu X G, Liu Q R, Huo G, et al 2012 Colloid Surf. A:Physicochem. Eng. Asp. 407 23
[6]	Li X Y, Si Z J, Lei Y Q, et al. 2011 Cryst. Eng. Comm. 13 642
[7]	Hao H Q, Ma Q M, He F, et al. 2014 J. Mater. Chem. B 2 7978
[8]	Ling Y, Tang X Z, Wang F J, et al. 2017 RSC Adv. 7 2913
[9]	Gu L, He X M, Wu Z Y 2014 Mater. Res. Bull. 59 65
[10]	Casula M F, Floris P, Innocenti C, et al. 2010 Chem. Mater. 22 1739
[11]	Shen L Z, Qiao Y S, Guo Y, et al. 2013 Optoelecyron. Adv. Mat. 7 525
[12]	Song L N, Zang F C, Song M J, et al. 2015 J. Nanosci. Nanotechno. 15 4111
[13]	Claire C, Philippe R, Jean M I, et al. 2006 Adv. Drug. Deliver. Rer. 58 1478
[14]	Alexion C, Amold W, Hulin P, et al. 2001 J. Magn. Magn. Mater. 225 187
[15]	Liu R T, Liu J, Tong J Q, et al. 2012 Prog. Nat. Sci. 22 31
[16]	Li Q 2010 Beijing Biomed. Eng. 29 308 (in Chinese)[李强 2010 北京生物医学工程 29 308]
[17]	Barakat N S 2009 Nanomedicine-UK 4 799
[18]	Frey N A, Peng S, Cheng K, et al. 2009 Chem. Soc. Rev. 38 2532
[19]	Qin R H, Jiang W, Liu H Y, et al. 2007 J. Funct. Mater. 6 902 (in Chinese)[秦润华, 姜炜, 刘宏英, 等 2007 功能材料 6 902]
[20]	Bo W, Song L, Li S H, et al. 2007 J. Chongqing Med. Univ. 32 922 (in Chinese)[柏玮, 宋琳, 李少林, 等 2007 重庆医科大学学报 32 922]
[21]	Zhang Y K, Luo C, Zhu C M 2011 J. Third Mil. Med. Univ. 33 1224 (in Chinese)[张玉坤, 罗聪, 朱朝敏 2011 第三军医大学学报 33 1224]

施引文献

[1]	Zhu M Y, Liu C, Bo W Q, Hu J W, Hu Y H, Jin H M, Wang S W, Li Y 2012 Acta Phys. Sin. 61 078106 (in Chinese)[朱明原, 刘聪, 薄伟强, 舒佳武, 胡业昊, 金红明, 王世伟, 李瑛 2012 物理学报 61 078106]
[2]	Zheng X C, Li X Y, He L H, et al. 2017 Chin. Phys. B 26 037502
[3]	Gholizadeh A, Jafari E 2017 J. Magn. Magn. Mater. 422 328
[4]	Liu R, Yang S C, Wang F, et al. 2012 ACS Appl. Mater. Inter. 4 1537
[5]	Lu X G, Liu Q R, Huo G, et al 2012 Colloid Surf. A:Physicochem. Eng. Asp. 407 23
[6]	Li X Y, Si Z J, Lei Y Q, et al. 2011 Cryst. Eng. Comm. 13 642
[7]	Hao H Q, Ma Q M, He F, et al. 2014 J. Mater. Chem. B 2 7978
[8]	Ling Y, Tang X Z, Wang F J, et al. 2017 RSC Adv. 7 2913
[9]	Gu L, He X M, Wu Z Y 2014 Mater. Res. Bull. 59 65
[10]	Casula M F, Floris P, Innocenti C, et al. 2010 Chem. Mater. 22 1739
[11]	Shen L Z, Qiao Y S, Guo Y, et al. 2013 Optoelecyron. Adv. Mat. 7 525
[12]	Song L N, Zang F C, Song M J, et al. 2015 J. Nanosci. Nanotechno. 15 4111
[13]	Claire C, Philippe R, Jean M I, et al. 2006 Adv. Drug. Deliver. Rer. 58 1478
[14]	Alexion C, Amold W, Hulin P, et al. 2001 J. Magn. Magn. Mater. 225 187
[15]	Liu R T, Liu J, Tong J Q, et al. 2012 Prog. Nat. Sci. 22 31
[16]	Li Q 2010 Beijing Biomed. Eng. 29 308 (in Chinese)[李强 2010 北京生物医学工程 29 308]
[17]	Barakat N S 2009 Nanomedicine-UK 4 799
[18]	Frey N A, Peng S, Cheng K, et al. 2009 Chem. Soc. Rev. 38 2532
[19]	Qin R H, Jiang W, Liu H Y, et al. 2007 J. Funct. Mater. 6 902 (in Chinese)[秦润华, 姜炜, 刘宏英, 等 2007 功能材料 6 902]
[20]	Bo W, Song L, Li S H, et al. 2007 J. Chongqing Med. Univ. 32 922 (in Chinese)[柏玮, 宋琳, 李少林, 等 2007 重庆医科大学学报 32 922]
[21]	Zhang Y K, Luo C, Zhu C M 2011 J. Third Mil. Med. Univ. 33 1224 (in Chinese)[张玉坤, 罗聪, 朱朝敏 2011 第三军医大学学报 33 1224]

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空心Fe3O4纳米微球的制备及超顺磁性

1. 山西大同大学固体物理研究所, 大同 037009;

2. 西安交通大学理学院, 物质非平衡合成与调控教育部重点实验室, 西安 710049;

3. 深圳大学材料学院, 深圳 518061

通信作者: 卢学刚, xglu@xjtu.edu.cn

基金项目:

国家自然科学基金（批准号：51172178）资助的课题.

收稿日期: 2018-03-30

修回日期: 2018-05-16

刊出日期: 2018-09-05

摘要: 采用水热控制合成法，以六水三氯化铁、柠檬酸三钠和尿素为原料，聚丙烯酰胺为稳定剂，200 ℃下反应12 h制备得到了超顺磁性空心Fe3O4纳米微球.通过X射线衍射仪、扫描电子显微镜、透射电子显微镜对样品的结构和形貌进行表征，并采用振动样品磁强计测试了样品的磁性能.结果表明：所得样品为具有尖晶石结构的Fe3O4纳米微球，尺寸为160 nm 左右，呈分等级结构，即整个微球由粒径约18 nm 的初级晶粒自组装堆叠而成；室温下表现为典型的超顺磁性，且饱和磁化强度为73.3 emu/g （1 emu/g=1 A m2/kg），这种高饱和磁化强度可以由其初级晶粒晶化程度高且粒径较大以及这种特殊的二次自组装结构进行解释.这种Fe3O4纳米微球为疏松多孔的空心球状结构，具有粒径分布均匀、分散性良好和超顺磁性的特点，在药物靶向输运和肿瘤热疗中有潜在的应用.

关键词:

Synthesis and superparamagnetism of Fe3O4 hollow nano-microspheres

1.
Institute of Solid State Physics, Shanxi Datong University, Datong 037009, China;

2.
MOE Key Laboratory for Non-Equilibrium Synthesis and Modulation of Condensed Matter, School of Science, Xi'an Jiaotong University, Xi'an 710049, China;

3.
College of Material Science and Engineering, Shenzhen University, Shenzhen 518061, China

Fund Project:

Project supported by the National Natural Science Foundation of China (Grant No. 51172178).

Received Date: 30 March 2018

Accepted Date: 16 May 2018

Published Online: 05 September 2018

Abstract: Fe3O4 nanomaterials have received great attention due to their many applications in tumor diagnosis and tumor heat therapy based on their good biocompatibility, magnetic targeting ability and superparamagnetic properties to avoid magnetic reunion in the process of magnetic targeting. Most of superparamagnetic nanoparticles obtained by traditional methods exhibit lower saturation magnetization (MS), because of their small particle sizes. Enlarging the particle size is favorable to increase the MS of magnetic particles. However, the superparamagnetism of the particle could be lost with the increase of particle size. This is not favorable to the targeting delivery of magnetic particles. For this purpose, in this paper, novel Fe3O4 nano-microspheres with mesoporous hollow structure are successfully synthesized by a facile hydrothermal method from the FeCl36 H2O, sodium citrate, urea, and polyacrylamide as additive, the reaction temperature is 200℃ and reaction time is 12 h. The crystal structure and purity of the resulting products are examined by powder X-ray diffraction (XRD). The morphologies of the products are studied by using scanning electron microscopy (SEM) and transmission electron microscopic (TEM). The magnetic properties of Fe3O4 nano-microspheres are evaluated with a vibrating sample magnetometer. The morphology evolution process and possible formation mechanism of Fe3O4 nano-microspheres are investigated. The findings are as follows:all XRD peaks of the hollow Fe3O4 nano-microspheres could be assigned to the spinel-type Fe3O4. The SEM and TEM images reveal that the products are mesoporous hollow Fe3O4 nano-microspheres and possess hierarchical structure, in which large microspheres (160 nm) are self-assembled by smaller Fe3O4 initial crystals (18 nm). It is found that the synthetic time of Fe3O4 nano-microspheres is considerable for the formation of the Fe3O4 hierarchical structure, and that the dispersion and sphericity of Fe3O4 nano-microspheres are the best when reaction time is 12 h. The formation of hierarchical hollow structure is believed to be due to the Ostwald ripening process, in which the initial crystals redissolve and regrow. Furthermore, the magnetic measurement results show that as-prepared hollow Fe3O4 nano-microspheres exhibit typical superparamagnetic properties whose initial crystal size is in the range of superparamagnetic region. Meanwhile, MS is about 73.3 emu/g at room temperature, which is significantly greater than that of traditional small superparamagnetic nanoparticles and compact solid nano-microspheres. The high saturation magnetization of hollow Fe3O4 nano-microspheres originates from a high crystallinity with primary grain, lager size and hierarchical structure. The results indicate that the as-prepared Fe3O4 hollow nano-microspheres are dispersed, water-soluble, homogeneous in particle diameter, and superparamagnetic, and can be used in targeted anticancer drug delivery and tumor heat therapy.

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